3-(2,4-Dichlorophenyl)propanoic acid → 4,6-Dichloro-1-indanone

HRID 430070

반응식

HRID 430070 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][C:11]([OH:13])=O>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]2[C:3]=1[CH2:9][CH2:10][C:11]2=[O:13]

참가 물질

3

실험 절차

3-(2,4-dichlorophenyl)propanoic acid (0.44 g, 2 mmol) in polyphosphoric acid (7 g) was heated to 100° C. under argon. After 90 min the mixture was cooled and treated with water (20 ml) and extracted with hexane (40 ml). The hexane layer was dried (MgSO4), and evaporated to dryness. The residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane to give the title product as a yellow solid, (0.018 g, 4.5%), δH (CDCl3) 2.8 (2H, m), 3.1 (2H, m), 7.6 (1H, d), 7.65 (1H, d).

후처리

  1. temperatureAfter 90 min the mixture was cooled
  2. extractionextracted with hexane (40 ml)
  3. dry with materialThe hexane layer was dried (MgSO4)
  4. customevaporated to dryness
  5. customThe residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane

출처 및 근거

ORD 기록
ord-bdaed1af101f4a3fb37531108d241fdc
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06320051B1

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